CN109813670B - Full-spectrum measurement method of mid-infrared light and corresponding device - Google Patents
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Abstract
The invention provides a full-spectrum measurement method of mid-infrared light, which comprises the following steps: the method comprises the following steps: the method comprises the steps that mid-infrared light and pump light are simultaneously projected onto at least two up-conversion crystals to generate sum frequency, the mid-infrared light is up-converted into visible light, and the sum of up-conversion wave bands of the at least two up-conversion crystals covers the full spectrum of the mid-infrared light; step two: detecting the converted visible light; and a third step: and obtaining the full spectrum of the mid-infrared light based on the detection result of the visible light. The full-spectrum measurement method of the mid-infrared light has the advantages of high resolution, high signal-to-noise ratio, high reading speed, high sensitivity and low cost.
Description
Technical Field
The invention belongs to the field of optical detection, and particularly relates to a full-spectrum measurement method of mid-infrared light and a corresponding device.
Background
The identification of the species of a substance by an infrared characteristic absorption peak is a very important analytical means in the fields of physics, chemistry, biology and medicine, and the principle is that the composition of chemical components of the substance is reflected by a vibration peak of infrared spectrum. The infrared spectrum detection method mainly adopts an infrared detector. Currently, infrared detectors are mainly classified into two types, i.e., thermal detectors and photon detectors according to detection mechanisms, wherein photon detectors are widely used in spectral measurement due to high sensitivity and short response time, and commercial high-sensitivity photon detectors mainly include two types, i.e., refrigeration type photon unit detectors and focal plane array detectors. When a photon unit detector is used for measuring a spectrum, different components of the spectrum are scanned by mainly rotating a grating through a spectrometer, and light intensities with different frequencies are obtained in sequence. In addition, for example, a Mercury Cadmium Telluride (MCT) focal plane array detector composed of a plurality of pixel points can rapidly perform one-time full spectrum measurement on a mid-infrared spectrum, but in order to reduce the dark current effect of a detector material, the detector needs to operate at a low temperature of 77K, and each pixel point needs to be connected with a corresponding signal amplification device to amplify a signal, so that the mid-infrared multichannel detector is large in size and expensive (more than 80 ten thousand RMB). The current Mercury Cadmium Telluride (MCT) array detector has low pixel number and uneven imaging quality of each pixel, which limits the resolution of signals. Meanwhile, the MCT array detector has a small number of pixel points, so that the single-shot spectrum range is narrow, and the detection of the broadband spectrum needs the splicing of a plurality of windows, so that the practical application of the MCT array detector is greatly limited. Therefore, there is a need to develop a mid-infrared full-spectrum detection technique with high resolution, high signal-to-noise ratio, high reading rate and low cost.
Disclosure of Invention
Therefore, the present invention is directed to overcome the above-mentioned drawbacks of the prior art, and provides a full spectrum measurement method for mid-infrared light, comprising the following steps:
the method comprises the following steps: the method comprises the steps that mid-infrared light and pump light are simultaneously projected onto at least two up-conversion crystals to generate sum frequency, the mid-infrared light is up-converted into visible light, and the sum of up-conversion wave bands of the at least two up-conversion crystals covers the full spectrum of the mid-infrared light;
step two: detecting the converted visible light; and
step three: and obtaining the full spectrum of the mid-infrared light based on the detection result of the visible light.
According to the full-spectrum measurement method of mid-infrared light, the full-spectrum waveband of the mid-infrared light is preferably 3 μm to 10 μm.
According to the full spectrum measurement method of mid-infrared light, one of the at least two up-conversion crystals is preferably MgO LiNbO3A crystal, another is AgGaGeS4And (4) crystals.
According to the full spectrum measurement method of mid-infrared light of the present invention, preferably, in the second step, the converted visible light is detected by using a linear array CMOS detector.
According to the full spectrum measurement method of mid-infrared light of the present invention, preferably, the step two includes the following sub-steps:
2-1: splitting the visible light; and
2-2: the visible light after light splitting passes through the linear array CMOS detector, so that the light intensity I of the visible light is obtainedsignalThe relationship of the change with the pixel point P.
According to the full spectrum measurement method of mid-infrared light of the present invention, preferably, the step three includes the following sub-steps:
3-1: fitting the wavelength λ of mid-infrared light with at least two characteristic absorption standards in a frequency window of the mid-infrared lightMIRA functional relationship with the pixel point P;
3-2: according to the intensity of visible light IsignalThe variation relation with the pixel point P and the wavelength lambda of the mid-infrared lightMIRObtaining the light intensity I of the mid-infrared light according to the functional relation with the pixel point PMIRWith the wavelength lambda of the mid-infrared lightMIRThe relationship (2) of (c).
According to the full spectrum measurement method of mid-infrared light of the present invention, preferably, the functional relationship is a linear functional relationship or a quadratic functional relationship.
The invention also provides a full-spectrum measuring device of mid-infrared light, which comprises:
the up-conversion component comprises at least two up-conversion crystals, and the sum of up-conversion wave bands of the at least two up-conversion crystals covers the full spectrum of mid-infrared light, wherein the mid-infrared light and the pump light are simultaneously projected onto the at least two up-conversion crystals to generate sum frequency, so that the mid-infrared light is up-converted into visible light;
the visible light detection component comprises a spectrometer and a visible light detector, wherein the visible light detector comprises a visible light detection module and a conversion module, the visible light detection module is used for detecting visible light split by the spectrometer, and the conversion module is used for converting the output of the visible light detection module into a spectrum of mid-infrared light.
According to the full-spectrum measuring device of mid-infrared light, the output of the visible light detection module is preferably the light intensity I of visible lightsignalThe relationship of the change with the pixel point P.
According to the full spectrum measurement device of mid-infrared light of the present invention, preferably, the conversion module further includes a fitting module for fitting a functional relationship between the wavelength of mid-infrared light and the pixel point.
Compared with the prior art, the invention has the advantages that: the visible light detector is used for full spectrum measurement of mid-infrared spectrum, and has high resolution, high signal-to-noise ratio, high reading speed, high sensitivity and low cost.
Drawings
Embodiments of the invention are further described below with reference to the accompanying drawings, in which:
FIG. 1 is a schematic diagram of an optical path for performing full spectrum measurement of mid-infrared light in accordance with an embodiment of the present invention;
fig. 2 is a schematic diagram of the upconversion principle according to the present invention;
FIG. 3 is a schematic diagram of frequency scaling using a standard of characteristic absorption;
FIG. 4 is a graph showing a comparison of a mid-infrared spectrum obtained by a visible light detector and a mid-infrared spectrum obtained by a single channel scan in accordance with the present invention;
FIG. 5 is a time resolved mid-IR spectrum of tungsten hexacarbonyl in cyclopentane solution; and
fig. 6A and 6B are two-dimensional infrared spectra of sodium azide obtained using single-channel mid-infrared detection and using the visible multi-channel detection of the present invention, respectively.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail by embodiments with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Fig. 1 is a schematic diagram illustrating a full spectrum measurement method of mid-infrared light according to an embodiment of the present invention, and fig. 1 is a schematic diagram illustrating an optical path for implementing the full spectrum measurement of mid-infrared light according to the embodiment of the present invention.
First, obtain mid-infrared light and pump light
Referring to fig. 1, a laser pulse having a center wavelength of 800nm generated by a femtosecond laser system 1 is reflected by a mirror M1 and then incident on a beam splitting sheet BS1, and the beam splitting sheet BS1 splits the light into a first laser beam B1 for generating pump light that is transmitted and a second laser beam B2 for generating mid-infrared light that is reflected. In this example, the transmission of the beam splitting sheet is 70%. First laserThe beam B1 is incident on the hollow mirror Rf1 fixed to the motorized stage via the mirror M2, and the optical path is adjusted in order to synchronize the pump light and mid-infrared light finally obtained to the up-conversion crystal. Emergent light of the hollow reflector Rf1 sequentially passes through the reflectors M3 and M4, then enters an 1800G/mm grating G1 placed at a certain depression angle, and different frequency components scattered by the grating are converged on a focal plane of the grating through a spherical mirror CM1 with the focal length of 500 nm. Placing a slit with adjustable width on the focal plane for obtaining the half-height width of 0.2nm (corresponding to the up-conversion resolution of 3 cm)-1) The central wavelength and the bandwidth of the pump light can be changed by adjusting the slit. In addition, to save space and enhance the stability of the system, a mirror M5 is placed behind the slit at the focal plane, so that the reflected light returns at an angle to the vertical direction of the original optical path and finally reaches the upconverting crystal in a broadened manner. Specifically, the limited narrowband pump light is reflected by the mirror M5 back to the spherical mirror, then reaches the diffraction grating, is reflected by the diffraction grating, then sequentially passes through the mirror M6 and the lens L1, and then is split by the semi-transparent semi-reflective beam splitting sheet BS2 to respectively reach the up-conversion crystals C1 and C2.
Referring also to FIG. 1, a second laser beam B2, previously obtained by a beam splitter BS1, is directed via a mirror M7 into the optical parametric amplifier 2 to produce a mid-infrared spectrum (about 300 cm) with a tunable center wavelength as desired-1Bandwidth) of the infrared light, or directly passing through an air spinning process to generate a broadband mid-infrared spectrum (3-10 μm).
And secondly, converting the mid-infrared light into visible light by using the sum frequency of the mid-infrared light and the pump light.
Specifically, with continued reference to FIG. 1, the mid-infrared light passes through a mirror M8 and a focusing lens L2 (CaF) in that order2Focal length 200mm) reaches the half-mirror BS3 to be split into two beams, and one beam passes through the mirror M9 and the half-mirror BS2 in this order to reach the upconversion crystal C1 (MgO: LiNbO3) The other beam sequentially passes through the reflectors M11 and M12 and the 800nm high-reflection film-coated calcium fluoride sheet M13 to reach the upconversion crystal C2 (AgGaGeS)4). Separately arriving upconversionMid-infrared light and pump light on crystals C1 and C2 sum. Specifically, the intermediate infrared light and the pump light in the wave band of 3-5 microns generate visible light at the neutralization frequency of the up-conversion crystal C1, and the intermediate infrared light and the pump light in the wave band of 5-10 microns generate visible light at the neutralization frequency of the up-conversion crystal C2, so that the intermediate infrared full spectrum is conveniently converted into visible light. When the up-conversion signal is adjusted, the space of the two beams of light is required to be adjusted to coincide with the time, the left and right inclination angles, the pitch angles and the in-plane rotation angles of the crystal are optimized, the maximum conversion efficiency of the signal is achieved, and the schematic diagram of the up-conversion principle is shown in an attached figure 2. The stretched 800nm laser is stretched in a time domain, and a sum frequency process is generated by femtosecond mid-infrared pulses, and the pulse width of the obtained visible light signal mainly depends on mid-infrared light. From the frequency domain, the broadened 800nm laser is actually a narrow-band pulse signal, and can generate sum frequency process with the broadband mid-infrared light, and the narrower the bandwidth of the 800nm narrow-band pulse, the higher the resolution of the mid-infrared up-conversion process.
And thirdly, detecting visible light.
With reference to fig. 1, the visible light signal obtained after the upconversion sequentially passes through a reflector M14 or M10 and M15, then is focused by a lens L3(NBK7, focal length is 50mm), is introduced into the spectrometer 3, is split by the visible light grating, is introduced into the linear array CMOS detector (imaging Solutions Group LW-ELIS-1394A, linear array pixel number is 1024, and single pixel size is 7.8um 125um), and obtains the light intensity I of the visible lightsignalWith the change relation of the pixel points P, the pixel points P correspond to the visible light frequency or the visible light frequency windows one by one.
IV, based on IsignalThe P relationship yields the full spectrum of mid-infrared light.
From the nonlinear optical frequency conversion relationship, the frequency ω of the pump light is knownupMid-infrared frequency omegaMIRAnd the frequency omega of visible lightsignalThe relationship of (1) is: omegaup+ωMIR＝ωsignalTherefore, the wave number of visible light obtained by up-converting 3-10 μm mid-infrared light by 800nm pump light is 13500cm-1-15833cm-1The corresponding visible light wavelength range is 631.6 nm-740.7 nm.
First, medium red is selectedThe external light frequency distribution window is calibrated to a standard sample with characteristic absorption at low, medium and high wave number (long, medium and short wave) peak positions. Fitting the functional relation between the intermediate infrared wavelength and the pixel points by using a binomial expression. Referring to fig. 3, fig. 3 is a schematic diagram of frequency scaling using a standard of characteristic absorption. And selecting three standard samples for calibration corresponding to the range of the mid-infrared window, wherein the wider the absorption frequency coverage of the three standard samples is, the more accurate the fitted curve is. In this example, sodium azide was used in dimethyl sulfoxide (2000.904 cm)-1) Sodium azide in heavy water (2043.278 cm)-1) And methyl thiocyanate in dimethylformamide (2154.736 cm)-1) The absorption peak in (1) is the standard peak position. The middle infrared absorption peaks and the corresponding pixel points of three standard samples are known, and the low-frequency absorption peak 1950cm-1Corresponding to the pixel point P1(200), the intermediate frequency absorption peak is 2050cm-1Corresponding pixel point P2(500), and high-frequency absorption peak 2150cm-1Corresponding to the pixel point P3(800), the wave number of the pump light is 1/800nm which is 12500cm-1From this, it can be calculated that the wave numbers of visible light after sum frequency are 14450cm each-1、14550cm-1And 14650cm-1The corresponding visible light wavelengths are 692.04nm, 687.29nm and 682.59nm, respectively. Respectively substituting the values of lambda 1, lambda 2, lambda 3, P1, P2 and P3 into a binomial fitting formula lambdaMIR＝aP2+ bP + c, and a-2.78E-7, b-1.60E-2, and c-6.95E 2 were calculated.
Known as IsignalP relation, λMIRP relation, ωsignal～ωMIRRelationship, also known as visible intensity IsignalAnd mid-infrared light intensity IMIRIs proportional, so the intermediate infrared light intensity I can be obtained by conversionMIRAnd mid-infrared frequency omegaMIRI.e. the spectrum of the mid-infrared light. Since the visible light is obtained by full-spectrum conversion of the mid-infrared light, a full spectrum of the mid-infrared light is finally obtained.
The conversion process is embedded into a CMOS visible light detector for frequency axis calibration, and then multi-channel full spectrum measurement of mid-infrared light can be realized. Compared with a single-channel acquisition mode, the method has the advantage that the data acquisition speed and the signal-to-noise ratio are greatly improved. Referring to fig. 4, fig. 4 shows a comparison of the mid-infrared spectrum acquired by the visible light detector according to the invention with the mid-infrared spectrum acquired by single channel scanning, it can be seen that the noise of the mid-infrared spectrum acquired by the method of the invention is significantly improved.
The method for detecting the mid-infrared spectrum by utilizing the room-temperature multi-channel visible light detector can be integrated into an ultra-fast mid-infrared spectrum acquisition system, and is synchronous with laser pulses in an external trigger mode, so that the acquisition of the ultra-fast infrared spectrum is realized. FIG. 5 shows a time-resolved mid-infrared spectrum (266nm pump-mid-infrared detection) of tungsten hexacarbonyl in cyclopentane solution, embodying the application of the present invention in one-dimensional ultra-fast infrared spectroscopy. Fig. 6A and 6B are two-dimensional infrared spectra of sodium azide corresponding to 250fs in heavy water obtained by single-channel mid-infrared detection and visible multi-channel detection according to the present invention, respectively, and fig. 6B is a graph in which the signal-to-noise ratio is improved by 20 times compared to fig. 6A and the data acquisition time is shortened to 1/90, which embodies the advantages of the mid-infrared full-spectrum measurement method according to the present invention, and can be applied to the current leading-edge two-dimensional infrared spectrum technology to detect molecular vibration modes.
In the above embodiment of the present invention, MgO capable of up-converting mid-infrared light of a wavelength band of 3 μm to 5 μm is used: LiNbO3Crystal and AgGaGeS capable of up-converting mid-infrared light with wave band of 5-10 mu m4The full spectrum of the mid-infrared light with the wavelength of 3-10 microns is simultaneously up-converted into visible light, then the visible light is detected by a visible light detector with lower cost and is converted into the spectrum of the mid-infrared light, and therefore the full spectrum measurement of the mid-infrared light with low cost, high speed, high resolution, high signal-to-noise ratio and high sensitivity is achieved.
According to other embodiments of the present invention, more than two upconversion crystals may be employed as long as the sum of the conversion bands of the individual upconversion crystals is able to cover the full spectrum of mid-infrared light.
According to other embodiments of the present invention, the pump light and the mid-infrared light are generated by different light sources, and in this case, the pump light source and the mid-infrared light source need to be coupled.
According to other embodiments of the present invention, when fitting the relationship between the frequency of the mid-infrared light and the pixel point, two standard samples are selected and implemented by linear fitting, or more than three standard samples are selected and implemented by higher-order fitting.
Although the present invention has been described by way of preferred embodiments, the present invention is not limited to the embodiments described herein, and various changes and modifications may be made without departing from the scope of the present invention.
Claims (10)
1. A full-spectrum measurement method of mid-infrared light comprises the following steps:
the method comprises the following steps: the method comprises the steps that mid-infrared light and pump light are simultaneously projected onto at least two up-conversion crystals to generate sum frequency, the mid-infrared light is up-converted into visible light, and the sum of up-conversion wave bands of the at least two up-conversion crystals covers the full spectrum of the mid-infrared light;
step two: detecting the converted visible light; and
step three: and obtaining the full spectrum of the mid-infrared light based on the detection result of the visible light.
2. The full-spectrum measurement method of mid-infrared light according to claim 1, wherein the full-spectrum band of mid-infrared light is 3 μm to 10 μm.
3. The method for full-spectrum measurement of mid-infrared light according to claim 1, wherein one of the at least two up-conversion crystals is MgO LiNbO3A crystal, another is AgGaGeS4And (4) crystals.
4. The full spectrum measurement method of mid-infrared light according to claim 3, wherein in step two, the converted visible light is detected by a linear array CMOS detector.
5. The full spectrum measurement method of mid-infrared light according to claim 4, wherein the second step includes the substeps of:
2-1: splitting the visible light; and
2-2: the visible light after light splitting passes through the linear array CMOS detector, so that the light intensity I of the visible light is obtainedsignalThe relationship of the change with the pixel point P.
6. The full spectrum measurement method of mid-infrared light according to claim 5, wherein the third step includes the substeps of:
3-1: fitting the wavelength λ of mid-infrared light with at least two characteristic absorption standards in a frequency window of the mid-infrared lightMIRA functional relationship with the pixel point P;
3-2: according to the intensity of visible light IsignalThe variation relation with the pixel point P and the wavelength lambda of the mid-infrared lightMIRObtaining the light intensity I of the mid-infrared light according to the functional relation with the pixel point PMIRWith the wavelength lambda of the mid-infrared lightMIRThe relationship (2) of (c).
7. The method for full spectrum measurement of mid-infrared light of claim 6, wherein the functional relationship is a linear functional relationship or a quadratic functional relationship.
8. A full-spectrum measurement device of mid-infrared light, comprising:
the up-conversion component comprises at least two up-conversion crystals, and the sum of up-conversion wave bands of the at least two up-conversion crystals covers the full spectrum of mid-infrared light, wherein the mid-infrared light and the pump light are simultaneously projected onto the at least two up-conversion crystals to generate sum frequency, so that the mid-infrared light is up-converted into visible light;
the visible light detection component comprises a spectrometer and a visible light detector, wherein the visible light detector comprises a visible light detection module and a conversion module, the visible light detection module is used for detecting visible light split by the spectrometer, and the conversion module is used for converting the output of the visible light detection module into a spectrum of mid-infrared light.
9. The method of claim 8, wherein the mid-infrared light is a mixture of infrared light and infrared lightThe spectrum measuring device, wherein the output of the visible light detection module is the light intensity I of the visible lightsignalThe relationship of the change with the pixel point P.
10. The mid-infrared full spectrum measurement apparatus of claim 9, wherein the conversion module further comprises a fitting module for fitting a functional relationship of the wavelength of the mid-infrared light to the pixel points.
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